CN114058837B - Method for preparing molybdenum oxide from molybdenite concentrate based on microwave roasting process - Google Patents

Method for preparing molybdenum oxide from molybdenite concentrate based on microwave roasting process Download PDF

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CN114058837B
CN114058837B CN202111395838.1A CN202111395838A CN114058837B CN 114058837 B CN114058837 B CN 114058837B CN 202111395838 A CN202111395838 A CN 202111395838A CN 114058837 B CN114058837 B CN 114058837B
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molybdenite concentrate
spheres
molybdenum
molybdenum oxide
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CN114058837A (en
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刘秉国
周俊文
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Kunming University of Science and Technology
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B1/00—Preliminary treatment of ores or scrap
    • C22B1/02—Roasting processes
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G39/00—Compounds of molybdenum
    • C01G39/02—Oxides; Hydroxides
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B1/00—Preliminary treatment of ores or scrap
    • C22B1/14—Agglomerating; Briquetting; Binding; Granulating
    • C22B1/24—Binding; Briquetting ; Granulating
    • C22B1/2406—Binding; Briquetting ; Granulating pelletizing
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B34/00—Obtaining refractory metals
    • C22B34/30—Obtaining chromium, molybdenum or tungsten
    • C22B34/34—Obtaining molybdenum
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/80—Compositional purity

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Abstract

The invention discloses a method for preparing molybdenum oxide from molybdenite concentrate based on a microwave roasting process, which belongs to the technical field of molybdenum metallurgy and comprises the following steps: (1) Crushing molybdenite concentrate into powder, adding sodium carbonate to prepare spheres, and drying; (2) Uniformly paving the spheres obtained in the step (1) in a ceramic crucible, and then placing the spheres in a cavity of a microwave reactor; (3) carrying out microwave roasting, and reacting for 20-50min at 200-350 ℃; (4) Heating to the sublimation temperature of 700-900 ℃ at the speed of 120-150 ℃/min, preserving the heat for 10-15min, overflowing molybdenum trioxide steam generated by oxidizing roasting through the top of a microwave reactor, cooling by water, and collecting by a cloth bag dust collector to obtain molybdenum oxide, wherein the purity of the prepared molybdenum trioxide is more than 99.95%, and the sulfur content is less than 0.005%.

Description

Method for preparing molybdenum oxide from molybdenite concentrate based on microwave roasting process
Technical Field
The invention relates to the technical field of molybdenum metallurgy, in particular to a method for preparing molybdenum oxide from molybdenite concentrate based on a microwave roasting process.
Background
The molybdenum element has a series of oxides, and the most stable of the oxides of molybdenum is molybdenum trioxide (MoO) 3 ) And molybdenum dioxide (MoO) 2 ) In addition, there are also some intermediate compounds having a valence between +6 and + 4. Molybdenum trioxide is light green or white powder, is an indispensable intermediate compound in the process of producing metal molybdenum, and occupies an important position in the molybdenum metallurgy industry. Molybdenum trioxide is used as an important molybdenum product, the known preparation method is a molybdenite oxidizing roasting-ammonia leaching method, and the main process of the method is to oxidize and roast molybdenite concentrate at 500-550 ℃ to obtain molybdenum calcine (the main component is MoO) 3 ) And then, carrying out ammonia leaching on the molybdenum calcine to obtain an ammonium molybdate solution, and then carrying out impurity removal, drying, crystallization and calcination on the ammonium molybdate solution to obtain the molybdenum trioxide. Although the process is mature, the process is complex, the flow is long, a large amount of heat energy and ammonia water are consumed in the production process, the cost is high, and the environmental pollution is large.
Zhang Qin Xiu et al provide a method for producing pure molybdenum trioxide by conventional roasting molybdenum foundry sand sublimation method (tungsten molybdenum metallurgy, 9 months 2005), although the molybdenum trioxide product can be obtained by direct roasting, the method has higher requirements for raw materials and cannot adapt to molybdenite raw ore; on the other hand, in the method, the sublimation temperature of the molybdenum foundry sand needs to be controlled between 900 and 1100 ℃, so that the molybdenum trioxide with the purity of 99.8 percent can be prepared, and the energy consumption is higher.
Therefore, how to shorten the molybdenum metallurgy process flow and reduce the energy consumption is a technical problem to be solved urgently by those skilled in the art.
Disclosure of Invention
The invention provides a method for preparing molybdenum oxide from molybdenite concentrate based on a microwave roasting process, aiming at the problems of complex process, long flow, high energy consumption, high roasting temperature and serious environmental pollution of the existing method for producing pure molybdenum trioxide from molybdenite concentrate.
In order to achieve the purpose, the invention provides the following scheme:
a method for preparing molybdenum oxide from molybdenite concentrate based on a microwave roasting process comprises the following steps:
(1) Crushing the molybdenite concentrate into powder, adding calcium oxide and sodium carbonate into the powder to prepare spheres, and drying the spheres;
(2) Uniformly paving the spheres obtained in the step (1) in a ceramic crucible, and then placing the spheres in a cavity of a microwave reactor;
(3) Microwave roasting, and reacting at 200-350 deg.C for 20-50min;
(4) Heating to a sublimation temperature of 700-900 ℃ at a speed of 120-150 ℃/min, preserving heat for 10-15min, overflowing molybdenum trioxide steam generated by oxidizing roasting through the top of the microwave reactor, cooling by water, and collecting by a bag dust collector to obtain high-purity molybdenum trioxide.
Further, the median particle size of the molybdenite concentrate powder in the step (1) is 1-3 μm.
Further, in the molybdenite concentrate in the step (1), the mass percentage of molybdenum is more than or equal to 52 percent, the sulfur content is less than or equal to 30 percent, the total content of copper is less than or equal to 0.1 percent, the total content of phosphorus, tin and lead is less than or equal to 0.2 percent, and the content of arsenic is less than or equal to 0.01 percent.
Further, the diameter of the sphere in the step (1) is 3-5mm.
Further, the addition amount of the calcium oxide in the step (1) is 5-10% of the weight of the molybdenite concentrate powder; the addition amount of the sodium carbonate is 0.05-0.1% of the weight of the molybdenite concentrate powder.
Furthermore, the spheres in the step (2) are built into 3-5 layers in the cavity of the microwave reactor, because the microwave energy can directly penetrate through a sample with a certain depth, the inside and the outside can be heated simultaneously, the heat transfer process is not needed, the specified temperature can be instantly reached, and the addition of the sodium carbonate can ensure that the microwave baking device can simultaneously perform microwave baking on the multilayer spheres, and the material thickness is not strictly limited like powder.
Further, oxygen is blown in during the microwave roasting process in the step (3).
Further, the oxygen bubbling amount in the step (3) is 3-12m 3 /h。
Further, the microwave power in the step (3) is 700-900W.
The invention discloses the following technical effects:
according to the method for preparing molybdenum oxide from molybdenite concentrate based on the microwave roasting process, molybdenite concentrate is prepared into spheres, calcium oxide is added and can react with silicon oxide to generate a slag phase, and molybdenum separation is accelerated; due to the addition of sodium carbonate, the roasting temperature in the microwave reaction process is remarkably reduced, the roasting time is also remarkably shortened, the problems of molybdenum volatilization loss and impurity sintering cannot be caused due to the lower roasting temperature, and the purity of the prepared molybdenum trioxide is over 99.95 percent and the sulfur content is below 0.005 percent.
Detailed Description
Reference will now be made in detail to various exemplary embodiments of the invention, the detailed description should not be construed as limiting the invention but as a more detailed description of certain aspects, features and embodiments of the invention.
It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. Further, for numerical ranges in this disclosure, it is understood that each intervening value, between the upper and lower limit of that range, is also specifically disclosed. Every smaller range between any stated value or intervening value in a stated range and any other stated or intervening value in a stated range is encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated by reference herein for the purpose of disclosing and describing the methods and/or materials associated with the documents. In case of conflict with any incorporated document, the present specification will control.
It will be apparent to those skilled in the art that various modifications and variations can be made in the specific embodiments of the present disclosure without departing from the scope or spirit of the disclosure. Other embodiments will be apparent to those skilled in the art from consideration of the specification. It is intended that the specification and examples be considered as exemplary only.
As used herein, the terms "comprising," "including," "having," "containing," and the like are open-ended terms that mean including but not limited to.
Example 1
Crushing molybdenite concentrate into powder with the median particle size of 1-3 mu m, wherein the main components and percentage content of the molybdenite concentrate are 57.16% of molybdenum, 28.15% of sulfur, 0.07% of copper, 0.021% of phosphorus, 0.02% of tin, 0.13% of lead and 0.005% of arsenic, adding sodium carbonate accounting for 0.05% of the mass of the powder and 6% of calcium oxide to prepare a sphere with the diameter of 3mm, drying until the water content is 10%, building 3 layers of the spheres and uniformly paving the spheres in a ceramic crucible, then placing the ceramic crucible in a cavity of a microwave reactor, and blowing in the ceramic crucible with the flow of 5m 3 And h, carrying out microwave roasting with 700W microwave power, reacting at 250 ℃ for 50min, heating to 750 ℃ at the speed of 150 ℃/min, keeping the temperature for 15min, overflowing molybdenum trioxide steam generated by oxidative roasting through the top of the microwave reactor, cooling by water, and collecting by a bag dust collector to obtain the high-purity molybdenum trioxide.
Through determination: the purity of the molybdenum trioxide is 99.95 percent, the sulfur content is 0.0048 percent, and the molybdenum recovery rate is 98.41 percent.
Example 2
The molybdenite concentrate is crushed into powder with the median particle size of 1-3 mu m, the main components and the percentage content of the molybdenite concentrate are similar to those of the example 1, sodium carbonate accounting for 0.05 percent of the mass of the powder and calcium oxide accounting for 5 percent of the mass of the powder are added to prepare spheres with the diameter of 5mm, the spheres are dried until the water content is 10 percent, 3 layers of the spheres are built and evenly paved in a ceramic crucible, and then the spheres are paved in 3 layersPlacing a ceramic crucible in a cavity of a microwave reactor, wherein the blowing flow is 10m 3 And h, carrying out microwave roasting on oxygen, wherein the microwave power is 800W, reacting for 20min at 300 ℃, heating to 800 ℃ at the speed of 150 ℃/min, keeping the temperature for 15min, overflowing molybdenum trioxide steam generated by oxidation roasting through the top of the microwave reactor, and collecting the molybdenum trioxide steam through a bag dust collector after water cooling to obtain the high-purity molybdenum trioxide.
Through determination: the purity of the molybdenum trioxide is 99.97 percent, the sulfur content is 0.0045 percent, and the molybdenum recovery rate is 98.82 percent.
Example 3
The molybdenite concentrate is crushed into powder with the median particle size of 1-3 mu m, the main components and the percentage content of the molybdenite concentrate are similar to those of the example 1, sodium carbonate accounting for 0.08 percent of the mass of the powder and calcium oxide accounting for 10 percent of the mass of the powder are added to prepare spheres with the diameter of 5mm, the spheres are dried until the water content is 10 percent, 5 layers of the spheres are built and evenly spread in a ceramic crucible, then the ceramic crucible is placed in a cavity of a microwave reactor, and the flow rate is 10m after the ceramic crucible is blown 3 And h, carrying out microwave roasting by using oxygen, wherein the microwave power is 900W, reacting for 40min at 300 ℃, heating to 800 ℃ at the speed of 150 ℃/min, keeping the temperature for 15min, overflowing molybdenum trioxide steam generated by oxidation roasting through the top of a microwave reactor, cooling by water, and collecting by using a cloth bag dust collector to obtain the high-purity molybdenum trioxide.
Through determination: the purity of the molybdenum trioxide is 99.98 percent, the sulfur content is 0.0041 percent, and the molybdenum recovery rate is 98.51 percent.
Example 4
Crushing molybdenite concentrate into powder with the median particle size of 1-3 mu m, wherein the main components and percentage content of the molybdenite concentrate are 53.17% of molybdenum, 29.51% of sulfur, 0.08% of copper, 0.015% of phosphorus, 0.02% of tin, 0.15% of lead and 0.004% of arsenic, adding sodium carbonate accounting for 0.1% of the mass of the powder and 8% of calcium oxide to prepare spheres with the diameter of 5mm, drying until the water content is 10%, building 5 layers of the spheres to be uniformly and flatly paved in a ceramic crucible, then placing the ceramic crucible in a cavity of a microwave reactor, and blowing in the ceramic crucible with the flow of 12m 3 H, carrying out microwave roasting with 800W of microwave power, reacting at 350 ℃ for 30min, heating to 800 ℃ at the speed of 150 ℃/min, keeping the temperature for 15min, and carrying out microwave reaction on molybdenum trioxide steam generated by oxidizing roastingOverflowing from the top of the device, and collecting the molybdenum trioxide with high purity by a cloth bag dust collector after water cooling.
Through determination: the purity of the molybdenum trioxide is 99.97 percent, the sulfur content is 0.0043 percent, and the molybdenum recovery rate is 98.95 percent.
Example 5
Crushing molybdenite concentrate into powder with a median particle size of 1-3 mu m, wherein the main components and percentage contents of molybdenite concentrate are 52.32% of molybdenum, 27.32% of sulfur, 0.08% of copper, 0.018% of phosphorus, 0.02% of tin, 0.12% of lead and 0.005% of arsenic, adding sodium carbonate accounting for 0.05% of the mass of the powder and 5% of calcium oxide to prepare spheres with a diameter of 5mm, drying until the water content is 10%, building 3 layers of the spheres, uniformly paving the spheres in a ceramic crucible, placing the ceramic crucible in a cavity of a microwave reactor, and blowing in a gas with a flow of 3m 3 And h, carrying out microwave roasting with 900W of oxygen gas, reacting at 300 ℃ for 20min, heating to 700 ℃ at the speed of 120 ℃/min, keeping the temperature for 10min, overflowing molybdenum trioxide steam generated by oxidative roasting through the top of the microwave reactor, cooling with water, and collecting by a cloth bag dust collector to obtain the high-purity molybdenum trioxide.
Through determination: the purity of the molybdenum trioxide is 99.96 percent, the sulfur content is 0.0047 percent, and the molybdenum recovery rate is 98.45 percent.
Comparative example 1
The difference is from example 1 only that no sodium carbonate is added.
Because sodium carbonate is not added, the content of the obtained molybdenum trioxide is less at a lower roasting temperature, and subsequent measurement is not carried out.
Comparative example 2
The same as example 1, except that only sodium carbonate was added in an amount of 10%.
The adding amount of the sodium carbonate is too high, which is not beneficial to the generation of the molybdenum trioxide, and the obtained molybdenum trioxide has less content and is not subjected to subsequent measurement.
Comparative example 3
The only difference from example 1 is that no calcium oxide was added.
In the same reaction time as in example 1, the separation of molybdenum was slow, which was not favorable for the production of molybdenum trioxide, and the obtained molybdenum trioxide was low in content and was not measured subsequently.
The above-described embodiments are only intended to illustrate the preferred embodiments of the present invention, and not to limit the scope of the present invention, and various modifications and improvements made to the technical solution of the present invention by those skilled in the art without departing from the spirit of the present invention should fall within the protection scope defined by the claims of the present invention.

Claims (5)

1. A method for preparing molybdenum oxide from molybdenite concentrate based on a microwave roasting process is characterized by comprising the following steps:
(1) Crushing the molybdenite concentrate into powder, adding calcium oxide and sodium carbonate into the powder to prepare spheres, and drying the spheres;
(2) Uniformly paving the spheres obtained in the step (1) in a ceramic crucible, and then placing the spheres in a cavity of a microwave reactor;
(3) Microwave roasting, and reacting at 200-350 deg.C for 20-50min;
(4) Heating to sublimation temperature of 700-900 deg.C at a rate of 120-150 deg.C/min, maintaining for 10-15min, allowing molybdenum trioxide vapor generated by oxidizing roasting to overflow from the top of the microwave reactor, cooling with water, and collecting with a bag collector to obtain molybdenum oxide;
the median particle size of the molybdenite concentrate powder in the step (1) is 1-3 mu m, and the addition amount of the calcium oxide in the step (1) is 5-10% of the mass of the molybdenite concentrate powder; the addition amount of the sodium carbonate is 0.05-0.1% of the weight of the molybdenite concentrate powder;
and (3) blowing oxygen in the microwave roasting process.
2. The method for preparing molybdenum oxide from molybdenite concentrates based on the microwave roasting process as claimed in claim 1, wherein the molybdenite concentrate of step (1) contains molybdenum in an amount of not less than 52% by mass, sulfur in an amount of not more than 30% by weight, copper in an amount of not more than 0.1% by weight, phosphorus, tin and lead in an amount of not more than 0.2% by weight, and arsenic in an amount of not more than 0.01% by weight.
3. The method for preparing molybdenum oxide from molybdenite concentrate based on microwave roasting process according to claim 1, wherein the diameter of the sphere in step (1) is 3-5mm.
4. The method for preparing molybdenum oxide from molybdenite concentrate based on microwave roasting process of claim 1, wherein the spheres of step (2) build 3-5 layers in the cavity of the microwave reactor.
5. The method for preparing molybdenum oxide from molybdenite concentrate based on microwave roasting process of claim 1, wherein the oxygen input in step (3) is 3-12m 3 /h。
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CN104326509B (en) * 2014-10-10 2016-06-22 昆明理工大学 A kind of microwave calcining molybdenite concentrate produces the method for high-pure molybdenum oxide
CN105112647B (en) * 2015-09-06 2017-12-05 中南大学 A kind of solid sulphur method of Low Grade Molybdenum Concentrates lime method roasting
CN105734265B (en) * 2016-03-09 2017-12-26 金堆城钼业股份有限公司 A kind of method that molybdenum concntrate removes silicon
CN108383163B (en) * 2017-03-30 2020-04-24 中南大学 Method for preparing high-purity molybdenum trioxide by roasting molybdenite concentrate in one step
CN107815535B (en) * 2017-10-26 2019-11-26 中南大学 A kind of method of microwave radiation exaraction molybdenum
CN107779590B (en) * 2017-10-31 2020-01-14 中南大学 Method for extracting molybdenum and rhenium
CN111926175B (en) * 2019-05-16 2021-06-25 中南大学 Method for extracting molybdenum trioxide by using molybdenum concentrate sulfur dioxide to assist calcification roasting
CN110065969B (en) * 2019-06-06 2021-02-05 中南大学 Method for preparing pure molybdenum trioxide by microwave roasting molybdenum concentrate pellets

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